摘要
目的建立血中氰离子的衍生化气相色谱-质谱联用(GC/MS)分析方法。方法血液样品依次加入苯胺的环己烷溶液、亚硝酸钠溶液以及盐酸溶液,涡旋混合。再加入硫酸铜溶液,混匀后放入50℃水浴加热15min。离子肼气质联用法(GC-MS/MS)检测衍生物苯甲腈和内标物氯代苄。采用标准品衍生物的标准质谱图定性分析,选择m/z76(苯甲腈二级质谱特征峰),m/z65(氯代苄二级质谱特征峰)作为定量离子进行定量分析。结果血中氰离子的最低检出限为0.05μg/mL,提取回收率为95%。结论该方法专属性强,操作简便,适用于血中氰离子检测。
Objective To establish a GC/MS/MS derivatization method for determining the cyanide in blood.Methods Blood sample was sequentially added with the solutions of aniline cyclohexane,sodium nitrite and hydrochloric acid,then being subjected to vortex for mixing.After one more addition of copper sulfate solution into the above sampling blood,the mixture was heated at 50℃ for 15 min,thus resulting in the benzyl cyanide/chloride to be determined by GC/MS/MS,with the ions m/z 76 and m/z 65 for quantitative analysis of characteristic peak from benzyl cyanide/chloride.Results The cyanide ions in blood sample showed the limit of detection as 0.05 μg/mL and the average recovery about 95%.Conclusion This method is of specificity,rapid for qualitative analysis of cyanide in blood.
作者
李想
朱昱
夏鑫鑫
LI Xiang;ZHU Yu;XIA Xinxin(National Criminal Investigative Police University of China,Shenyang 110854,China)
出处
《刑事技术》
2019年第3期254-256,共3页
Forensic Science and Technology
